EP0100266B1 - Procédé de préparation d'un mélange à base de trichlorosilane utilisable pour la préparation de silicium de haute pureté - Google Patents

Procédé de préparation d'un mélange à base de trichlorosilane utilisable pour la préparation de silicium de haute pureté Download PDF

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Publication number
EP0100266B1
EP0100266B1 EP83401454A EP83401454A EP0100266B1 EP 0100266 B1 EP0100266 B1 EP 0100266B1 EP 83401454 A EP83401454 A EP 83401454A EP 83401454 A EP83401454 A EP 83401454A EP 0100266 B1 EP0100266 B1 EP 0100266B1
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EP
European Patent Office
Prior art keywords
trichlorosilane
reaction
gas
plasma
silicon tetrachloride
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP83401454A
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German (de)
English (en)
French (fr)
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EP0100266A1 (fr
Inventor
Jean-Luc Lepage
Gérard Simon
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rhodia Chimie SAS
Original Assignee
Rhone Poulenc Specialites Chimiques
Rhone Poulenc Chimie SA
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Application filed by Rhone Poulenc Specialites Chimiques, Rhone Poulenc Chimie SA filed Critical Rhone Poulenc Specialites Chimiques
Publication of EP0100266A1 publication Critical patent/EP0100266A1/fr
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Publication of EP0100266B1 publication Critical patent/EP0100266B1/fr
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S423/00—Chemistry of inorganic compounds
    • Y10S423/09—Reaction techniques
    • Y10S423/10—Plasma energized

Definitions

  • the present invention relates to a process for the preparation of a mixture based on trichlorosilane which can be used for the preparation of high purity silicon.
  • This trichlorosilane during its decomposition, leads to the formation of significant quantities of silicon tetrachloride, the decomposition of the trichlorosilane taking place according to the reaction 4HSiCl 3 Si + 3 SiC14 + 2 H2.
  • silane SiH 4 by disproportionation of trichlorosilane also leads to the formation of silicon tetrachloride which it is necessary to recycle in the state of trichlorosilane.
  • This reaction must be carried out at a temperature between 250 and 350 ° C and in the presence of a catalyst consisting of copper or a copper-based alloy. It has been found that, using this reaction, it was possible not only to produce a new quantity of trichlorosilane, to also produce hydrogen which will be recycled, but also to react all of the hydrochloric acid contained in the reaction gas, so that the purification of the gas obtained, with a view to the decomposition of the trichlorosilane which it contains, no longer poses any problem. Finally, the calories necessary to initiate the reaction of hydrochloric acid on silicon will advantageously come from the previous reaction of reduction of silicon tetrachloride in plasma medium.
  • quenching means a gas different from the plasma gas such as vaporized SiCl 4 or a third inert gas in the medium.
  • This gas is sent to the reactor 6 which also receives silicon powder 7; the temperature in this reactor is between 250 and 350 ° C and small quantities of copper powder are also admitted.
  • the temperature in this reactor is between 250 and 350 ° C and small quantities of copper powder are also admitted.
  • This gas is sent to a column 10 where, by washing, one separates, on the one hand, the permanent gases (plasma gas) which can be recycled, and, on the other hand, the silicon products which leave at 11.
  • the permanent gases plasma gas
  • the silicon products which leave at 11.
  • These are optionally purified if they contain traces of HCl and then the decomposition of the trichlorosilane is optionally carried out under known conditions.
  • the plasma jet is produced by a blown arc generator with a power of 12.5KW.
  • the cathode is made up of a 10mm diameter thorium tungsten bar with a conical shape.
  • the anode is made of copper and has the shape of a nozzle 4mm in diameter and 38mm long, flared on the cathode side.
  • the plasma gas is a hydrogen argon mixture in the volume ratio 3/7. Its flow rate is 401 / min. The voltage is 62.5V and the intensity has been set at 200 A.
  • reaction vaporized silicon tetrachloride is injected directly at the outlet of the nozzle. Its flow rate is 4.31 / h (in liquid form).
  • the quenching gas consists of silicon tetrachloride in gaseous form. Its temperature is 120-125 ° C. It is injected 40mm from the injection point of the reaction silicon tetrachloride, its flow rate is 8.61 / h (in liquid form).
  • a probe located in the axis of the plasma generator allows samples to be taken for chromatographic analysis of the gas mixture obtained. Cooling is limited to 50 ° C to avoid condensation of the silicon tetrachloride.
  • composition of this mixture at the outlet of the reactor is as follows:
  • the conversion rate of the reactional silicon tetrachloride into trichlorosilane is 50.4% and the energy consumption, calculated taking into account the flow rates and the power of the plasma torch, is 4.9KWh per kg of trichlorosilane formed.
  • the plasma gas is sent to the same plasma generator (identical intensity and voltage).
  • reaction silicon tetrachloride is injected at a rate of 4.31 / h (in liquid form).
  • the quenching gas consists of methane, its flow rate is 30 l / min.
  • composition of the gas mixture leaving the reactor is as follows:
  • the complement to 100 consists of various silanes.
  • this composition corresponds to a conversion rate of silicon tetrachloride of 64.5%.
  • the yield of trichlorosilane relative to transformed SiCl 4 is 85.4%.
  • the energy consumption is 4.5 kWh per kg of trichlorosilane formed.
  • a mixture of 20 g of silicon powder (average diameter 100 microns) and 2.26 g of metallic copper powder was used as solid filler.
  • the mixture is admitted to a reactor (fixed bed) and heated to 300 ° C; a gaseous reagent is sent to this mixture, the molar composition of which is as follows:
  • the flow rate of this gas is 2.251 / h.
  • Example 3 is repeated by operating at 260 ° C. with a gas of the following molar composition:
  • the plasma generator is identical to that of Example 1.
  • the plasma gas is a hydrogen argon mixture in the volume ratio 35/65. Its flow rate is 401 / min. The voltage is 70V and the intensity of 200 A.
  • the silicon tetrachloride is injected, in vaporized form, at a rate of 4.21 / h (liquid rate), or 0.607 moles / min.
  • the quenching gas consisting of argon is injected; 45mm from the injection point of silicon tetrachloride, at a flow rate of 251 / min.
  • the molar composition of the gas mixture leaving the reactor is as follows:
  • This composition corresponds to a conversion rate of hydrochloric acid equal to 100% with a selectivity equal to 97.1% in trichlorosilane and 2.9% in silicon tetrachloride.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
EP83401454A 1982-07-26 1983-07-13 Procédé de préparation d'un mélange à base de trichlorosilane utilisable pour la préparation de silicium de haute pureté Expired EP0100266B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8212971A FR2530638A1 (fr) 1982-07-26 1982-07-26 Procede de preparation d'un melange a base de trichlorosilane utilisable pour la preparation de silicium de haute purete
FR8212971 1982-07-26

Publications (2)

Publication Number Publication Date
EP0100266A1 EP0100266A1 (fr) 1984-02-08
EP0100266B1 true EP0100266B1 (fr) 1987-04-29

Family

ID=9276302

Family Applications (1)

Application Number Title Priority Date Filing Date
EP83401454A Expired EP0100266B1 (fr) 1982-07-26 1983-07-13 Procédé de préparation d'un mélange à base de trichlorosilane utilisable pour la préparation de silicium de haute pureté

Country Status (6)

Country Link
US (1) US4836997A (enrdf_load_stackoverflow)
EP (1) EP0100266B1 (enrdf_load_stackoverflow)
JP (1) JPS5945920A (enrdf_load_stackoverflow)
CA (1) CA1210221A (enrdf_load_stackoverflow)
DE (1) DE3371190D1 (enrdf_load_stackoverflow)
FR (1) FR2530638A1 (enrdf_load_stackoverflow)

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US5422088A (en) * 1994-01-28 1995-06-06 Hemlock Semiconductor Corporation Process for hydrogenation of tetrachlorosilane
US5869017A (en) * 1997-05-12 1999-02-09 Tokuyama Corporation Method of producing trichlorosilane having a reduced content of dichlorosilane
RU2142909C1 (ru) * 1998-07-30 1999-12-20 Институт химии высокочистых веществ РАН Способ получения высокочистого трихлорсилана и устройство для его осуществления
KR100385947B1 (ko) * 2000-12-06 2003-06-02 삼성전자주식회사 원자층 증착 방법에 의한 박막 형성 방법
DE102005005044A1 (de) * 2005-02-03 2006-08-10 Consortium für elektrochemische Industrie GmbH Verfahren zur Herstellung von Trichlorsilan mittels thermischer Hydrierung von Siliciumtetrachlorid
DE102005024041A1 (de) * 2005-05-25 2006-11-30 City Solar Ag Verfahren zur Herstellung von Silicium aus Halogensilanen
DE102005041137A1 (de) * 2005-08-30 2007-03-01 Degussa Ag Reaktor, Anlage und großtechnisches Verfahren zur kontinuierlichen Herstellung von hochreinem Siliciumtetrachlorid oder hochreinem Germaniumtetrachlorid
DE102006043929B4 (de) * 2006-09-14 2016-10-06 Spawnt Private S.À.R.L. Verfahren zur Herstellung von festen Polysilanmischungen
JP5601438B2 (ja) * 2006-11-07 2014-10-08 三菱マテリアル株式会社 トリクロロシランの製造方法およびトリクロロシラン製造装置
RU2350558C2 (ru) * 2007-05-02 2009-03-27 Федеральное государственное унитарное предприятие "Горно-химический комбинат" Способ получения трихлорсилана плазмохимическим гидрированием тетрахлорида кремния и устройство для его осуществления
DE102007041803A1 (de) * 2007-08-30 2009-03-05 Pv Silicon Forschungs Und Produktions Gmbh Verfahren zur Herstellung von polykristallinen Siliziumstäben und polykristalliner Siliziumstab
WO2010108065A1 (en) * 2009-03-19 2010-09-23 Ae Polysilicon Corporation Silicide - coated metal surfaces and methods of utilizing same
EP2421640A1 (en) * 2009-04-20 2012-02-29 Ae Polysilicon Corporation Methods and system for cooling a reaction effluent gas
KR20120023678A (ko) * 2009-04-20 2012-03-13 에이이 폴리실리콘 코포레이션 고순도 폴리실리콘의 제조를 위한 방법 및 장치
WO2010123873A1 (en) * 2009-04-20 2010-10-28 Ae Polysilicon Corporation A reactor with silicide-coated metal surfaces
KR20100117025A (ko) * 2009-04-23 2010-11-02 스미또모 가가꾸 가부시키가이샤 포토레지스트 패턴 형성 방법
DE102009037155B3 (de) * 2009-08-04 2010-11-04 Schmid Silicon Technology Gmbh Verfahren und Anlage zur Herstellung von Trichlorsilan
KR20120124061A (ko) 2010-01-26 2012-11-12 다우 코닝 코포레이션 오가노할로실란의 제조 방법
US8772525B2 (en) 2010-05-28 2014-07-08 Dow Corning Corporation Method for preparing a diorganodihalosilane
JP2013527203A (ja) 2010-05-28 2013-06-27 ダウ コーニング コーポレーション 有機ハロシランの調製
WO2012033644A1 (en) 2010-09-08 2012-03-15 Dow Corning Corporation Method for preparing a trihalosilane
DE102010044755A1 (de) 2010-09-08 2012-03-08 Spawnt Private S.À.R.L. Verfahren zur Herstellung von Silicium hoher Reinheit
BR112013014581A2 (pt) 2010-12-17 2019-09-24 Dow Corning método para a fabricação de um diorgano-di-halossilano
CN103261207B (zh) 2010-12-17 2015-09-23 道康宁公司 制备三卤代硅烷的方法
RU2013125229A (ru) 2011-01-25 2015-03-10 Дау Корнинг Корпорейшн Способ получения диорганодигалогенсилана
EP2768774B1 (en) * 2011-10-20 2017-03-22 REC Silicon Inc Fouling reduction in hydrochlorosilane production
US20150030520A1 (en) * 2012-03-14 2015-01-29 Centrotherm Photovoltaics Usa, Inc. Trichlorosilane production
FR2991988B1 (fr) 2012-06-15 2015-08-07 Laurent Laroche Procede de preparation d'objets en hydrogel biocompatible pour leur application dans le domaine medical, et plus particulierement en ophtalmologie
CN104736547A (zh) 2012-08-13 2015-06-24 道康宁公司 通过使氢、卤硅烷和有机卤化物在铜催化剂上以两步法反应制备有机卤硅烷的方法
EP2909217B1 (en) 2012-10-16 2016-10-26 Dow Corning Corporation Method of preparing halogenated silahydrocarbylenes
DE102013207444A1 (de) * 2013-04-24 2014-10-30 Evonik Degussa Gmbh Verfahren und Vorrichtung zur Herstellung von Polychlorsilanen
CN105705507B (zh) 2013-11-12 2018-08-31 美国陶氏有机硅公司 制备卤代硅烷的方法
WO2016099690A1 (en) 2014-12-18 2016-06-23 Dow Corning Corporation Method for producing aryl-functional silanes
CN112573522B (zh) * 2020-12-14 2022-07-26 亚洲硅业(青海)股份有限公司 硅基电子特气的制备方法及硅基电子特气的生产系统
CN113072074A (zh) * 2021-04-25 2021-07-06 森松（江苏）重工有限公司 还原炉的炉筒冷却方法、装置及多晶硅还原生产方法
CN113912066A (zh) * 2021-09-09 2022-01-11 全椒亚格泰电子新材料科技有限公司 一种制备氯代硅烷的方法

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GB883326A (en) * 1959-04-08 1961-11-29 Bbc Brown Boveri & Cie Method of producing trichlorsilane
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DE3024319C2 (de) * 1980-06-27 1983-07-21 Wacker-Chemitronic Gesellschaft für Elektronik-Grundstoffe mbH, 8263 Burghausen Kontinuierliches Verfahren zur Herstellung von Trichlorsilan
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US4451436A (en) * 1983-02-01 1984-05-29 Hare Louis R O Nitrogen fixation by plasma and catalyst

Also Published As

Publication number Publication date
DE3371190D1 (en) 1987-06-04
JPS6261530B2 (enrdf_load_stackoverflow) 1987-12-22
EP0100266A1 (fr) 1984-02-08
FR2530638B1 (enrdf_load_stackoverflow) 1985-02-22
JPS5945920A (ja) 1984-03-15
CA1210221A (fr) 1986-08-26
US4836997A (en) 1989-06-06
FR2530638A1 (fr) 1984-01-27

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